CN107963664A - A kind of thick VOCl3Prepare high-purity V2O5System and method - Google Patents

A kind of thick VOCl3Prepare high-purity V2O5System and method Download PDF

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Publication number
CN107963664A
CN107963664A CN201711330072.2A CN201711330072A CN107963664A CN 107963664 A CN107963664 A CN 107963664A CN 201711330072 A CN201711330072 A CN 201711330072A CN 107963664 A CN107963664 A CN 107963664A
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vocl
gas
storage tank
thick
ticl
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韩志彪
冯鲁兴
唐敬坤
张学伟
刘亮
员晓
吴道洪
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Jiangsu Province Metallurgical Design Institute Co Ltd
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Jiangsu Province Metallurgical Design Institute Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Inorganic Chemistry (AREA)
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Abstract

The present invention provides a kind of thick VOCl3Prepare high-purity V2O5System, which generally includes rectifying and removes SiCl4Device, VOCl3Storage tank, except TiCl4Device, essence VOCl3Storage tank, raw material preheating device, oxidation reaction apparatus, oxidizing gas feeding mechanism and V2O5Collection device.Present invention also offers a kind of thick VOCl3Prepare high-purity V2O5Method.V is prepared using the system and method for the present invention2O5, VOCl greatly improved3Purity, gained V2O5The purity of product can bring up to more than 99.9%, and flow significantly shortens and easy to automate, not produce waste water, and tail gas can be very suitable for docking with the technique of carburizing chlorination containing vanadium raw materials and produced high-purity V with reuse again after treatment2O5。

Description

A kind of thick VOCl3Prepare high-purity V2O5System and method
Technical field
The present invention relates to chemical field, and relate more specifically to a kind of thick VOCl3Prepare high-purity V2O5System and side Method.
Background technology
Traditional process for extracting vanadium is that the vanadium in vanadium-containing material is oxidized to high-valence state as far as possible, and is converted into soluble vanadic acid Salt (roasting, oxygen pressure acidleach etc.).Containing vanadium solution V is obtained by purification, precipitation, calcining2O5Product, gained V2O5Purity only have 98% or so, far from the requirement for meeting the high-tech sectors such as fine chemistry industry and flow battery.Containing vanadium raw materials, such as vanadium slag adds carbon Chlorination has the advantages of selectivity is strong, and reaction temperature is low, and reaction speed is fast, is widely used in vanadium titanium field of metallurgy.The flow Output purity is 80% or so thick VOCl3.However, the TiO in vanadium slag2Also can whole chlorinations, generate TiCl4Into thick VOCl3 In, seriously affect VOCl3And V2O5The purity of product.
The content of the invention
In view of this situation, the present invention provides a kind of thick VOCl3Prepare high-purity V2O5System and method.
According to an aspect of the present invention, there is provided a kind of thick VOCl3Prepare high-purity V2O5System, which includes：
Rectifying removes SiCl4Device, it includes thick VOCl3Feeding mechanism, rectifying column and equipment for steam treatment；
VOCl3Storage tank, VOCl3The feed inlet of storage tank is connected to the outlet at bottom of rectifying column；
Except TiCl4Device, except TiCl4The feed inlet of device is connected to VOCl3The discharge port of storage tank；
Smart VOCl3Storage tank, smart VOCl3The feed inlet of storage tank is connected to except TiCl4The discharge port of device；
Raw material preheating device, the feed inlet of raw material preheating device are connected to smart VOCl3The discharge port of storage tank；
Oxidation reaction apparatus, a feed inlet of oxidation reaction apparatus and the discharge port of raw material preheating device connect, another Feed inlet is connected with oxidizing gas feeding mechanism；
Oxidizing gas feeding mechanism, oxidizing gas feeding mechanism, which provides, to be used to aoxidize VOCl3Gas；
V2O5Collection device, V2O5Collection device is used for the V for collecting generation2O5。
According to one embodiment of present invention, the rectifying enriching section number of plates is 6~9 pieces, and the number of plates of stripping section is 10~20 pieces.
According to one embodiment of present invention, raw material preheating device is preheating furnace, and oxidation reaction apparatus is oxidation furnace, oxidation Another preheater is equipped between stove and oxidizing gas feeding mechanism.
According to one embodiment of present invention, V2O5Collection device includes cyclone separator and bagroom.
According to one embodiment of present invention, system further includes circulation of tail gas device, and it is cold that circulation of tail gas device includes tail gas But device and circulation line, the air inlet of exhaust gas cooler and the gas outlet of bagroom connect, the gas outlet of exhaust gas cooler It is connected with the air inlet and/or oxidizing gas feeding mechanism of bagroom.
According to another aspect of the present invention, there is provided one kind prepares high-purity V using said system2O5Method, this method includes The following steps：
1) by thick VOCl3Thick VOCl in feeding mechanism3It is transported in rectifying column and carries out rectification process, removes thick VOCl3 In SiCl4Impurity；
2) SiCl will be removed4VOCl afterwards3It is collected into VOCl3In storage tank；
3) by VOCl3VOCl in storage tank3It is transported to and removes TiCl4In device, to except TiCl4POCl is added in device3, TiCl4And POCl3Pressure filtration is carried out after fully combining, filtrate is collected into smart VOCl3In storage tank；
4) by smart VOCl3VOCl in storage tank3It is transported in raw material preheating device and is preheated；
5) by the VOCl after preheating3It is transported in oxidation reaction apparatus, and oxic gas is passed through into oxidation reaction apparatus Body, makes both react and generates V2O5；
6) flue gas after reaction in step 5) is drained into V2O5In collection device, V therein is collected2O5Powder.
According to one embodiment of present invention, rectification temperature is 70~90 DEG C wherein in step 1), and pressure is normal pressure, rectifying The reflux ratio of operation is 20~35.
According to one embodiment of present invention, wherein in step 4) by raw material preheating to 200~300 DEG C.
According to one embodiment of present invention, wherein this method further includes the oxidizing gas in step 5) being passed through oxidation The pre-heat treatment is first carried out before reaction unit, the temperature after oxidizing gas preheating is 200~300 DEG C, and oxidizing gas includes oxygen Gas and inert gas, the volume flow ratio for being passed through each gas in oxidation unit are VOCl3:O2:Inert gas=100:(83~ 90):(0~20).
According to one embodiment of present invention, the operating pressure control of wherein oxidation unit is 0.1~0.15MPa, oxidation The operating temperature of device is controlled at 700~900 DEG C.
By using the systems and methods of the present invention, following multiple beneficial effect can be obtained：
(1) present invention is with vanadium slag or the thick VOCl of bone coal chlorination output3For raw material, after refined, it will be most difficult to what is removed TiCl4Impurity removes, and VOCl greatly improved3Purity, gained V2O5The purity of product can bring up to more than 99.9%；
(2) with it is traditional roast containing vanadium raw materials-leach process for extracting vanadium compared with, be not required to purify by vanadium liquid, extract, precipitation, The a series of complex processes such as calcining, flow significantly shorten and easy to automate, do not produce waste water, and tail gas is after treatment again It can be very suitable for docking the high-purity V of production with the technique of carburizing chlorination containing vanadium raw materials with reuse2O5。
Brief description of the drawings
Fig. 1 shows the structure diagram of the system according to the present invention；
Fig. 2 shows the flow diagram of the method according to the invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to specific embodiment and attached Figure, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only explaining this hair It is bright, it is not intended to limit the present invention.
As shown in Figure 1, the thick VOCl of the present invention3Prepare high-purity V2O5System remove SiCl including rectifying4Device, VOCl3Storage Tank 12, except TiCl4Device 13, essence VOCl3Storage tank 14, raw material preheating device 15, oxidation reaction apparatus 19, oxidizing gas supply dress Put and V2O5Collection device.
Wherein rectifying removes SiCl4Device includes thick VOCl3Feeding mechanism, rectifying column 3 and equipment for steam treatment.Thick VOCl3 Feeding mechanism includes thick VOCl3Head tank 1, thick VOCl3Storage tank 2 and liquid sulfur pump.Equipment for steam treatment includes condenser 4, reflux Liquid collecting tank 5, containing VOCl3Silicon tetrachloride storage tank 6, rectifying section acid seal tank 7, tail gas leaching device 8 and air-introduced machine 9.Wherein, rectifying The portion gas discharged in tower 3 is condensed to liquid by condenser 4, is partly back to rectifying column 3 through phegma collecting tank 5, Remainder enters and contains VOCl3Silicon tetrachloride storage tank 6 in.The lack of gas produced in storage tank 6 are sent to tail after rectifying section acid seal tank 7 In gas leaching device 8.The gas that tail gas leaching device 8 is discharged after aqueous slkali absorption processing empties after air-introduced machine 9 is sent into chimney 10.
3 lower part of rectifying column can set distillation still 11.Distillate can be circulated back in rectifying column 3 through distillation still 11.Essence Evaporate the outlet at bottom and VOCl of tower 33Storage tank 12 is connected.VOCl3Storage tank 12 is used to collect and store to remove SiCl4VOCl3, its Still contain impurity TiCl4, therefore preparing V as raw material2O5Need further to remove TiCl therein before4。
VOCl3The discharge port of storage tank is with removing TiCl4The feed inlet connection of device 13.Except TiCl4Device includes reaction and purifies Tower, POCl3Storage tank, N2Purifier and VOCl3Condense refining plant.POCl3Storage tank, VOCl3Storage tank is purified to reaction respectively The POCl of addition scheduled volume in tower3With thick VOCl3, the two is combined into solid TiCl in reaction purifying column4·POCl3With TiCl4·2POCl3.Treat to be passed through N at the top of the backward reaction purifying column of fully reaction2Pressure filtration is carried out, filtrate is collected and will volatilize VOCl3Gas is condensed into liquid.The VOCl being collected into3Liquid is placed in smart VOCl3It is spare in storage tank 14.
Smart VOCl3The discharge port of storage tank 14 is connected with raw material preheating device 15 (such as preheating furnace), raw material preheating device 15 By smart VOCl3It is heated to 200~300 DEG C and is passed through oxidation furnace 19 after being allowed to gasification, is preheated to 200~300 DEG C and on the one hand realizes VOCl3Gasification, on the other hand, also avoid that preheating temperature is excessive, and initial reaction is excessively violent.Meanwhile by O2And inert gas Mixed gas 200~300 DEG C are heated in preheater 17 and is passed through in oxidation furnace 19, O2Excessive 10~20%.Use inertia Gas is as O2Diluent, avoid using pure O2The excessively fierce operation for being unfavorable for safety and stability of reaction.
The VOCl of heat3And O2+N2The reaction generation V in oxidation furnace 192O5.Two kinds of reactants are all in gas phase, easy to mix simultaneously Rapid reaction.Since the reaction can release substantial amounts of heat, once being just enough to maintain to react lasting progress, external heat is not required to Source.
The gas main component discharged from oxidation furnace 19 is V2O5And Cl2, the flue gas after reaction is discharged into V2O5Collection device. In embodiment shown in Fig. 1, V2O5Collection device is made of cyclone separator 20 and bagroom 21.Flue gas divides into whirlwind From device 20, most V is isolated2O5Powder, the flue gas come out from cyclone dust collectors 20 still contain a small amount of V2O5, then through cloth Bag collector 21 collects V2O5, the V that is collected into2O5It is placed in V2O5In storage tank 23.Because of the flue-gas temperature discharged from cyclone dust collectors 20 It is higher, therefore be passed through the cold tail gas in part before bag filter is entered from the flue gas of cyclone dust collectors discharge and cooled down, temperature Degree is down to less than 250 DEG C, and that bagroom 21 is collected into is solid-state V2O5Powder, obtains high-purity V2O5Purity it is reachable More than 99.9%.
In a preferred embodiment of the invention, which further includes circulation of tail gas utilization and exhaust gas processing device.From The tail gas main component that bagroom 21 is discharged is Cl2, at the same time containing a small amount of O2And inert gas.Tail gas after gathering dust passes through Freezing pressurization-rectifying can isolate more than 95% Cl2, available for preparing VOCl3, O2With the mixed gas one of inert gas Aspect can be directed to before bag filter 21 through wind turbine 25, mixed with 20 exiting flue gas of cyclone dust collectors, make to enter cloth bag The temperature of deduster 21 reduces, on the other hand with O2With the accumulation of inert gas, O2Oxidation furnace is also can return to inert gas, As VOCl3The raw material of oxidation reaction, at the same time, also mitigates the load of exhaust treatment system 26.
Fig. 2 shows that the present invention's prepares high-purity V2O5Method.
Thick VOCl is removed by rectificating method first3In SiCl4Impurity.The rectifying section number of plates of distillation operation is 6~9 Block, the number of plates of stripping section is 10~20 pieces, 70~90 DEG C of rectification temperature, and pressure is normal pressure, and the reflux ratio of distillation operation is 20 ~35.
POCl is introduced afterwards3To remove thick VOCl3In TiCl4Impurity.If thick VOCl3The quality of TiCl4 point in raw material Number is more than 0.1%, then needs to carry out except titanium operates.
Except titanium technique is as follows：
(1)POCl3With TiCl4Reaction generation TiCl4·POCl3、TiCl4·2POCl3
POCl3With thick VOCl3Respectively retort, POCl are introduced through flowmeter by respective storage tank3With VOCl3Reaction generation VOCl3·POCl3、VOCl3·2POCl3, control POCl3And VOCl3The molar ratio of impurity is (1.02~1.06):1, reaction temperature To spend for 40~60 DEG C, increase stirring in reaction process, agitator speed be 50~200 turns/min, mixing time is 20~ 40min, agitator speed are 50~200 turns/min, and 120~240min is stood after stirring, promote POCl3And TiCl4Impurity Fully it is combined into solid TiCl4·POCl3And TiCl4·2POCl3。
(2) pressure filtration
By the pressurized filtering of product, separation of solid and liquid is realized, obtained TiCl4·POCl3And TiCl4·2POCl3, through steaming Hair, TiCl4·POCl3And TiCl4·2POCl3It can be analyzed to TiCl4And POCl3, TiCl4And POCl3It is gaseous state, it is condensed, TiCl can be separately recovered4And POCl3。
(3) condensation is refined
The VOCl that previous step is obtained by filtration3Gas phase is cooled to 5~15 DEG C by solution with brine ice, is promoted in gas phase VOCl3Liquid is fully condensed into, to provide VOCl3The rate of recovery.
Thick VOCl3Remove TiCl4Obtain refined VOCl3Solution.
The smart VOCl that will be obtained3200~300 DEG C are preheating to preheating furnace, VOCl3Gasification, then passes to oxidation furnace, at the same time By O2200~300 DEG C, which are also preheating to, with the gaseous mixture of inert gas then passes to oxidation furnace.It is preheated to 200-300 DEG C of one side Realize VOCl3Gasification, on the other hand, also avoids that preheating temperature is excessive, and initial reaction is excessively violent.
VOCl3It is oxidized by oxygen as V2O5And release substantial amounts of heat.To improve VOCl3And O2Reaction effect in oxidation furnace Rate, fully improves the dynamic conditions of chemical reaction, and reactant is preheating to required temperature, O by the present invention respectively using preheater2 Excessive 10~20%, oxidation furnace is then passed to, two kinds of reactants are all in gas phase, easy to mix and react rapidly.The present invention is with lazy Property gas is as O2Diluent, avoid using pure O2Reaction it is excessively fierce, be unfavorable for the operation of safety and stability.Oxidation furnace 19 Operating pressure be 0.1~0.15MPa, the operating temperature of oxidation furnace is controlled 700 by adjusting the total flow of feed stock for blast furnace ~900 DEG C.The volume flow ratio for being passed through each gas of oxidation furnace is VOCl3:O2:Inert gas=100:(83~90):(0~20), Wherein inert gas includes but not limited to Ar, N2, He etc. any chemical reaction does not occur under normal running conditions in oxidation furnace Gas.The preferred Ar of the present invention.
Finally collect from oxidation furnace discharge gas (main component is V2O5And Cl2) in V2O5, obtain high-purity V2O5's Purity is up to more than 99.9%.
Below with the system and method for the specific embodiment description present invention.
Embodiment 1
By thick VOCl3SiCl is taken off successively4、TiCl4Refined VOCl is obtained afterwards3, the burner of preheater 17 is lighted, opens valve Door C is simultaneously passed through O2And N2Start to preheat, make O2+N2The temperature of mixed gas reaches 200 ± 5 DEG C, and mixing is determined by thermometer 18 The temperature of gas is met the requirements.Valve A is opened at the same time, is closed valve B, is lighted the burner of preheater 15 and be passed through smart VOCl3Open Begin to preheat, by smart VOCl3Temperature control at 200 ± 5 DEG C, VOCl is determined by thermometer 163Temperature meet the requirements after, beat Valve opening door B closes valve A, and opens the wind turbine of dust-precipitator 21, VOCl3Gas is passed through oxidation furnace 19, and oxygen-nitrogen mixture contact And oxidation reaction occurs.The volume flow ratio for the gas being passed through in oxidation furnace 19 is VOCl3:O2:N2=100:83:10, oxidation furnace 19 operating pressure is 0.1MPa, and the operating temperature of oxidation furnace 19 is controlled at 700 DEG C.The high-temperature flue gas warp come out from oxidation furnace 19 Cyclone dust collectors 20 isolate most V2O5Powder.The flue gas and O that cyclone dust collectors 20 export2+N2Cooling air-flow mixing drop Temperature collects solid-state V to less than 250 DEG C, from rotoclone collector 20 and bagroom 222O5Powder.Tail gas main component is Cl2, Contain a small amount of O at the same time2And N2, may separate out Cl after treatment2For the carburizing chlorination technique containing vanadium raw materials, the tail after gathering dust Gas can isolate more than 95% Cl by freezing pressurization-rectifying2, available for preparing VOCl3, O2And N2Mixed gas one Aspect can be directed to before bag filter 21 through wind turbine 25, mixed with 20 exiting flue gas of cyclone dust collectors, reduce flue gas temperature Degree.
The solid-state V collected using above-mentioned technique from rotoclone collector 20 and bagroom 222O5The purity of powder is reachable 99.92%.
Embodiment 2
By thick VOCl3SiCl is taken off successively4、TiCl4Refined VOCl is obtained afterwards3, the burner of preheater 17 is lighted, opens valve Door C is simultaneously passed through O2Start to preheat with Ar, make O2The temperature of+Ar mixed gas reaches 300 ± 5 DEG C, and mixing is determined by thermometer 18 The temperature of gas is met the requirements.Valve A is opened at the same time, is closed valve B, is lighted the burner of preheater 15 and be passed through smart VOCl3Open Begin to preheat, by smart VOCl3Temperature control at 300 ± 5 DEG C, VOCl is determined by thermometer 163Temperature meet the requirements after, beat Valve opening door B closes valve A, and opens the wind turbine of dust-precipitator 21, VOCl3Gas is passed through oxidation furnace 19, and the argon-mixed contact of oxygen And oxidation reaction occurs.The volume flow ratio for the gas being passed through in oxidation furnace 19 is VOCl3:O2:Ar=100:90:20, oxidation furnace 19 operating pressure is 0.15MPa, and the operating temperature of oxidation furnace 19 is controlled at 900 DEG C.The high-temperature flue gas come out from oxidation furnace 19 Most V is isolated through cyclone dust collectors 202O5Powder.The flue gas and O that cyclone dust collectors 20 export2+ Ar cooling air-flows mix Less than 250 DEG C are cooled to, solid-state V is collected from rotoclone collector 20 and bagroom 222O5Powder.Tail gas main component is Cl2, at the same time containing a small amount of O2And Ar, it may separate out Cl after treatment2For the carburizing chlorination technique containing vanadium raw materials, after gathering dust Tail gas by freezing pressurization-rectifying can isolate more than 95% Cl2, available for preparing VOCl3, O2With the gaseous mixture of Ar On the one hand body can be directed to before bag filter 21 through wind turbine 25, mixed with 20 exiting flue gas of cyclone dust collectors, reduce cigarette Temperature degree.
The solid-state V collected using above-mentioned technique from rotoclone collector 20 and bagroom 222O5The purity of powder is reachable 99.96%.
Embodiment 3
By thick VOCl3SiCl is taken off successively4、TiCl4Refined VOCl is obtained afterwards3, the burner of preheater 17 is lighted, opens valve Door C is simultaneously passed through O2Start to preheat with Ar, make O2The temperature of+Ar mixed gas reaches 250 ± 5 DEG C, and mixing is determined by thermometer 18 The temperature of gas is met the requirements.Valve A is opened at the same time, is closed valve B, is lighted the burner of preheater 15 and be passed through smart VOCl3Open Begin to preheat, by smart VOCl3Temperature control at 250 ± 5 DEG C, VOCl is determined by thermometer 163Temperature meet the requirements after, beat Valve opening door B closes valve A, and opens the wind turbine of dust-precipitator 21, VOCl3Gas is passed through oxidation furnace 19, and the argon-mixed contact of oxygen And oxidation reaction occurs.The volume flow ratio for the gas being passed through in oxidation furnace 19 is VOCl3:O2:Ar=100:87:15, oxidation furnace 19 operating pressure is 0.13MPa, and the operating temperature of oxidation furnace 19 is controlled at 900 DEG C.The high-temperature flue gas come out from oxidation furnace 19 Most V is isolated through cyclone dust collectors 202O5Powder.The flue gas and O that cyclone dust collectors 20 export2+ Ar cooling air-flows mix Less than 250 DEG C are cooled to, solid-state V is collected from rotoclone collector 20 and bagroom 222O5Powder.Tail gas main component is Cl2, at the same time containing a small amount of O2And Ar, it may separate out Cl after treatment2For the carburizing chlorination technique containing vanadium raw materials, after gathering dust Tail gas by freezing pressurization-rectifying can isolate more than 95% Cl2, available for preparing VOCl3, O2With the gaseous mixture of Ar On the one hand body can be directed to before bag filter 21 through wind turbine 25, mixed with 20 exiting flue gas of cyclone dust collectors, reduce cigarette Temperature degree.
The solid-state V collected using above-mentioned technique from rotoclone collector 20 and bagroom 222O5The purity of powder is reachable 99.98%.
Embodiment described above only expresses embodiments of the present invention, its description is more specific and detailed, but can not Therefore it is interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that for those of ordinary skill in the art, Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection model of the present invention Enclose.

Claims (10)

  1. A kind of 1. thick VOCl3Prepare high-purity V2O5System, it is characterised in that the system comprises：
    Rectifying removes SiCl4Device, it includes thick VOCl3Feeding mechanism, rectifying column and equipment for steam treatment；
    VOCl3Storage tank, the VOCl3The feed inlet of storage tank is connected to the outlet at bottom of rectifying column；
    Except TiCl4Device, it is described to remove TiCl4The feed inlet of device is connected to VOCl3The discharge port of storage tank；
    Smart VOCl3Storage tank, the essence VOCl3The feed inlet of storage tank is connected to except TiCl4The discharge port of device；
    Raw material preheating device, the feed inlet of the raw material preheating device are connected to smart VOCl3The discharge port of storage tank；
    Oxidation reaction apparatus, a feed inlet of the oxidation reaction apparatus and the discharge port of raw material preheating device connect, another Feed inlet is connected with oxidizing gas feeding mechanism；
    Oxidizing gas feeding mechanism, the oxidizing gas feeding mechanism, which provides, to be used to aoxidize VOCl3Gas；
    V2O5Collection device, the V2O5Collection device is used for the V for collecting generation2O5。
  2. 2. system according to claim 1, it is characterised in that the rectifying enriching section number of plates is 6~9 pieces, stripping section The number of plates be 10~20 pieces.
  3. 3. system according to claim 1, it is characterised in that raw material preheating device is preheating furnace, and oxidation reaction apparatus is Oxidation furnace, is equipped with another preheater between oxidation furnace and oxidizing gas feeding mechanism.
  4. 4. system according to claim 1, it is characterised in that V2O5Collection device includes cyclone separator and bag collection Device.
  5. 5. system according to claim 4, it is characterised in that the system also includes circulation of tail gas device, the tail gas Circulator includes exhaust gas cooler and circulation line, and the air inlet of exhaust gas cooler and the gas outlet of bagroom connect, The gas outlet of exhaust gas cooler and the air inlet of bagroom and/or oxidizing gas feeding mechanism connect.
  6. 6. a kind of system using as described in claim 1-5 prepares high-purity V2O5Method, it is characterised in that include following step Suddenly：
    1) by thick VOCl3Thick VOCl in feeding mechanism3It is transported in rectifying column and carries out rectification process, removes thick VOCl3In SiCl4Impurity；
    2) SiCl will be removed4VOCl afterwards3It is collected into VOCl3In storage tank；
    3) by VOCl3VOCl in storage tank3It is transported to and removes TiCl4In device, to except TiCl4POCl is added in device3, in TiCl4 And POCl3Pressure filtration is carried out after fully combining, filtrate is collected into smart VOCl3In storage tank；
    4) by smart VOCl3VOCl in storage tank3It is transported in raw material preheating device and is preheated；
    5) by the VOCl after preheating3It is transported in oxidation reaction apparatus, and oxidizing gas is passed through into oxidation reaction apparatus, makes Both, which react, generates V2O5；
    6) flue gas after reaction in step 5) is drained into V2O5In collection device, V therein is collected2O5Powder.
  7. 7. according to the method described in claim 6, it is characterized in that, rectification temperature is 70~90 DEG C in step 1), pressure is normal Pressure, the reflux ratio of distillation operation is 20~35.
  8. 8. according to the method described in claim 6, it is characterized in that, by raw material preheating to 200~300 DEG C in step 4).
  9. 9. according to the method described in claim 6, it is characterized in that, the method further includes that the oxidizing gas in step 5) exists The pre-heat treatment is first carried out before being passed through oxidation reaction apparatus, the temperature after oxidizing gas preheating is 200~300 DEG C, oxidizing gas Include oxygen and inert gas, the volume flow ratio for being passed through each gas in oxidation unit is VOCl3:O2:Inert gas=100: (83~90):(0~20).
  10. 10. according to the method described in claim 6, it is characterized in that, the operating pressure control of oxidation unit for 0.1~ 0.15MPa, the operating temperature of oxidation unit are controlled at 700~900 DEG C.
CN201711330072.2A 2017-12-13 2017-12-13 A kind of thick VOCl3Prepare high-purity V2O5System and method Pending CN107963664A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114380332A (en) * 2021-12-28 2022-04-22 攀钢集团攀枝花钢铁研究院有限公司 Method for purifying crude vanadium oxychloride

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114380332A (en) * 2021-12-28 2022-04-22 攀钢集团攀枝花钢铁研究院有限公司 Method for purifying crude vanadium oxychloride
CN114380332B (en) * 2021-12-28 2024-01-26 攀钢集团攀枝花钢铁研究院有限公司 Method for purifying crude vanadium oxychloride

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